CN103980811A - Efficient antibacterial waterborne polyurethane floor coating and preparation method thereof - Google Patents
Efficient antibacterial waterborne polyurethane floor coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an efficient antibacterial waterborne polyurethane floor coating and a preparation method thereof. The method comprises the following steps: firstly, reacting 1,6-hexamethylene diisocyanate (HDI) with polyether polyol, DMPA, a chain extender and the like to obtain a polyurethane prepolymer; then adding triethylamine for neutralization; adding an appropriate amount of auxiliaries and a waterborne antibacterial agent, and emulsifying at high speed to obtain the waterborne polyurethane floor coating. The waterborne polyurethane floor coating has excellent weather resistance, wear resistance and anti-microbial-adsorption performance. The waterborne polyurethane floor coating not only keeps good adhesive force to the floor, good water resistance and good chemicals resisting performance, but also has good antibacterial performance.
Description
Technical field
The present invention relates to a kind of high-efficiency antimicrobial aqueous polyurethane coating and preparation method thereof, belong to macromolecule material preparation area.
Background technology
Polyurethane coating because of it, film there is good wear resistance, the advantage such as erosion resistance, chemical-resistant, hardness are large, snappiness, and composition regulation is flexible, furniture application, anti-corrosion of metal, painting dressing automobiles, aircraft skin, hard floor paint, traffic paint etc. have been widely used in.
At present the polyurethane coating of China be take two-pack alcohol acid and polyurethane coating as main, and such coating is to make with the Synolac of TDI prepolymer and hydroxyl, but because of its yellowing serious, can only be for the indoor coating of dark color.Along with the development of technology, the especially growth of high-decoration weather-resistant coating demand, adopts the aliphatic polyurethane raw material of not yellowing, to improve yellowing, improves weathering resistance.For the aliphatic isocyanates of coating, mainly contain hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI), '-diphenylmethane diisocyanate (HMDI) and derivative thereof, consumption maximum be HDI type.
Along with growth in the living standard, people have higher requirement to the quality of living environment and health level, particularly to healthy consciousness also in continuous enhancing.On the other hand, various pathogenic microorganisms are very extensive in distributed in nature, and grow under certain condition, breed, and even variation not only can cause the decomposition, rotten and corrupt of various materials, the health that is also threatening the mankind.Therefore impel polyurethane coating hydrotropismsization, there is anti-microbial property future development.
Aqueous polyurethane coating is to take waterborne polyurethane resin as basis, the coating that the water of take is prepared as dispersion medium, there is the advantages such as toxicity is little, nonflammable, free from environmental pollution, energy-conservation, safe, some performances also with solvent borne polyurethane coating simultaneously, polyurethane coating hardness is high, strong adhesion, wear resistance, snappiness are good etc., and advantage combines with the low VOC of water-borne coatings.But, what aqueous polyurethane antibiotic paint was studied now is fewer, because, present antiseptic-germicide is mainly divided into inorganic antiseptic, organic antibacterial agent and complex antimicrobials, the mutual solubility of these antiseptic-germicides and water is not fine, therefore, if these antiseptic-germicides are joined and make antibiotic paint in aqueous polyurethane coating and can have certain difficulty.Therefore, exploitation has excellent weathering resistance, environmental protection, antibacterial aqueous polyurethane coating and has very important practical significance and potential value.
Summary of the invention
The invention provides a kind of high-efficiency antimicrobial aqueous polyurethane terrace paint and preparation method thereof, to solve the above-mentioned problems in the prior art.
For achieving the above object, the technical solution used in the present invention is as follows:
A high-efficiency antimicrobial aqueous polyurethane terrace paint, comprises A component and B component, it is characterized in that, described A component (isocyanate component) is comprised of the following raw material of counting by weight:
Described B component (curing agent component) is comprised of the following raw material of counting by weight:
Wherein, the preparation method of described aqueous high molecular bag carrying nano silver antiseptic-germicide is: first by polyoxyethylene glycol, epoxy resin is carried out to modification, obtain water miscible modified epoxy, then described water miscible modified epoxy is not only as reductive agent but also as stablizer, water is reaction medium, and the method for reduction Silver Nitrate has obtained the water-base epoxy bag Ag-carried antibacterial agent emulsion of stably dispersing.
As preferred version, described polyether glycol is selected from the polyether glycol that at least one degree of unsaturation in the multipolymer of polyglycol ether, polypropylene glycol ether, polyglycerol ether, polypentaerythritol ether, PTMG, above-mentioned several polyether glycols is 1～4.
As preferred version, described color stuffing comprises at least one in silicon powder, titanium dioxide, talcum powder, wollastonite powder, calcium carbonate, barium sulfate, kaolin.
As preferred version, described chainextender comprises amine chain extender and alcohols chainextender.
As further preferred version, described amine chain extender is selected from diethyl toluene diamine, diformazan sulfydryl tolylene diamine, N, at least one in N '-di-sec-butyl methylene dianiline (MDA); Described alcohols chainextender is selected from least one in BDO, 1,3 butylene glycol, TriMethylolPropane(TMP), glycerol, tetramethylolmethane.
As preferred version, described auxiliary agent is selected from least one in defoamer, thickening material, Ricinate, slip(ping)agent, flow agent.
A preparation method for high-efficiency antimicrobial aqueous polyurethane terrace paint as claimed in claim 1, it comprises the steps:
The preparation method of described A component comprises the steps: under nitrogen protection, by 1, react hexamethylene-diisocyanate and polyether glycol mixing post-heating to 85～95 ℃, then adds dimethylol propionic acid reaction 1h, finally adds chainextender, 55～65 ℃ of reaction 4～6h, cooling rear discharging, obtains isocyanic ester performed polymer, by described isocyanic ester performed polymer with in triethylamine and after, add again water-based bag Ag-carried antibacterial agent emulsion 10-30 weight part and deionized water, obtain A component product;
The preparation method of described B component comprises the steps: color stuffing, polyether glycol, chainextender, auxiliary agent, fire retardant to add in deionized water and mix, being ground to particle diameter is 30～50um, add again mill base, under the rotating speed of 700～1500rpm, stir and obtain B component, obtain B component product.
The invention has the advantages that: the aqueous polyurethane antibiotic paint making, compressive property reaches 75MPa, and extensibility reaches 27%; Weathering resistance is more than 10 years; Antibacterial aqueous polyurethane floor coatings antibacterium performance reaches 99%, and antibacterium endurance quality reaches 95%.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
In the present invention, the preparation method of water-based bag carrying silver antimicrobials used is: first by polyoxyethylene glycol, epoxy resin is carried out to modification, obtain water miscible epoxy resin, then described water-soluble epoxy resin is not only as reductive agent but also as stablizer, water is reaction medium, the method of reduction Silver Nitrate has obtained the aqueous high molecular bag carrying nano silver antiseptic-germicide of stably dispersing, i.e. water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide.
Embodiment 1
The preparation of A component: by the polyglycol ether of 25 weight parts, 1 of 25 weight parts, hexamethylene-diisocyanate (HDI) joins thermometer is housed, in the there-necked flask of whipping appts and reflux condensing tube, under nitrogen protection, be heated to 90 ℃ of reaction 2h, then the dimethylol propionic acid DMPA reaction 1h that adds 5 weight parts, finally add 7 weight part chainextender diethyl toluene diamines, 60 ℃ of reaction 4h, be cooled to 30 ℃ of dischargings, triethylamine for performed polymer (TEA) is neutralized to pH=7, add again water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide 2 weight parts, deionized water 30 weight parts, emulsify at a high speed 30min obtains white emulsion.
The preparation of B component: add silicon powder 10 weight parts, titanium dioxide 8 weight parts, talcum powder 8 weight parts in Scattered Kettle, polyglycol ether 30 weight parts, deionized water 25 weight parts, TriMethylolPropane(TMP) 5 weight parts, silicone antifoam agent 2 weight parts, polyether modified silicon oil flow agent 1 weight part, poly carboxylic acid ammonium salt dispersion agent 2 weight parts, middling speed disperses, after 1h, then through sand mill, to be ground to granularity at 30～50um.In mixture, add mill base 9 weight parts again, high speed dispersion evenly obtains B component.
During use, B component is joined in component A by the weight ratio of 1:1, high-speed stirring 15min under normal temperature, with trowel or Cylinder coating brush in accomplishing fluently on the terrace of priming paint.
Embodiment 2
The preparation of A component: by the polypropylene glycol ether of 22 weight parts, 1 of 28 weight parts, hexamethylene-diisocyanate (HDI) joins thermometer is housed, in the there-necked flask of whipping appts and reflux condensing tube, under nitrogen protection, be heated to 90 ℃ of reaction 2h, then the dimethylol propionic acid DMPA reaction 1h that adds 7 weight parts, finally add 4 weight part chainextender diformazan sulfydryl tolylene diamines, 60 ℃ of reaction 3h, be cooled to 30 ℃ of dischargings, triethylamine for performed polymer (TEA) is neutralized to pH=7, add again water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide 1 weight part, deionized water 30 weight parts, emulsify at a high speed 10min obtains white emulsion.
The preparation of B component: add silicon powder 8 weight parts, titanium dioxide 10 weight parts, talcum powder 10 weight parts in Scattered Kettle, polypentaerythritol ether 25 weight parts, deionized water 25 weight parts, TriMethylolPropane(TMP) 5 weight parts, silicone antifoam agent 2 weight parts, polyether modified silicon oil flow agent 2 weight parts, poly carboxylic acid ammonium salt dispersion agent 3 weight parts, fire retardant Sodium Tetraborate 2 weight parts, middling speed disperses, after 1.5h, then through sand mill, to be ground to granularity at 30um.In mixture, add mill base 10 weight parts again, high speed dispersion evenly obtains B component.
During use, B component is joined in component A by the weight ratio of 1:1.2, high-speed stirring 15min under normal temperature, with trowel or Cylinder coating brush in accomplishing fluently on the terrace of priming paint.
Embodiment 3
The preparation of A component: by the PCDL of 30 weight parts, 1 of 26 weight parts, hexamethylene-diisocyanate (HDI) joins thermometer is housed, in the there-necked flask of whipping appts and reflux condensing tube, under nitrogen protection, be heated to 80 ℃ of reaction 3h, then the dimethylol propionic acid DMPA reaction 1h that adds 5 weight parts, finally add 5 weight part chainextenders 1, 4-butyleneglycol, 60 ℃ of reaction 5h, be cooled to 25 ℃ of dischargings, triethylamine for performed polymer (TEA) is neutralized to pH=7, add again water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide 1 weight part, deionized water 30 weight parts, emulsify at a high speed 30min obtains white emulsion.
The preparation of B component: add silicon powder 10 weight parts, titanium dioxide 8 weight parts, talcum powder 10 weight parts in Scattered Kettle, PTMG 25 weight parts, deionized water 30 weight parts, TriMethylolPropane(TMP) 4 weight parts, silicone antifoam agent 2 weight parts, polyether modified silicon oil flow agent 2 weight parts, poly carboxylic acid ammonium salt dispersion agent 2 weight parts, fire retardant calcium hydroxide 3 weight parts, middling speed disperses, after 2h, then through sand mill, to be ground to granularity at 30um.In mixture, add mill base 7 weight parts again, high speed dispersion evenly obtains B component.
During use, B component is joined in component A by the weight ratio of 1:1, high-speed stirring 15min under normal temperature, with trowel or Cylinder coating brush in accomplishing fluently on the terrace of priming paint.
Embodiment 4
The preparation of A component: by the polyglycerol ether of 40 weight parts, 1 of 25 weight parts, hexamethylene-diisocyanate (HDI) joins thermometer is housed, in the there-necked flask of whipping appts and reflux condensing tube, under nitrogen protection, be heated to 55 ℃ of reaction 2h, then the dimethylol propionic acid DMPA reaction 1h that adds 3 weight parts, finally add 4 weight part chainextender diethyl toluene diamines, 60 ℃ of reaction 4h, be cooled to 30 ℃ of dischargings, triethylamine for performed polymer (TEA) is neutralized to pH=7, add again water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide 2 weight parts, deionized water 20 weight parts, emulsify at a high speed 40min obtains white emulsion.
The preparation of B component: add silicon powder 15 weight parts, titanium dioxide 10 weight parts, talcum powder 12 weight parts in Scattered Kettle, polyglycerol ether 25 weight parts, deionized water 25 weight parts, TriMethylolPropane(TMP) 2 weight parts, silicone antifoam agent 2 weight parts, polyether modified silicon oil flow agent 2 weight parts, poly carboxylic acid ammonium salt dispersion agent 2 weight parts, ammonium polyphosphate flame retardant 3 weight parts, middling speed disperses, after 2h, then through sand mill, to be ground to granularity at 30um.In mixture, add mill base 5 weight parts again, high speed dispersion evenly obtains B component.
During use, B component is joined in component A by the weight ratio of 1.5:1, high-speed stirring 20min under normal temperature, with trowel or Cylinder coating brush in accomplishing fluently on the terrace of priming paint.
Embodiment 5
The preparation of A component: by the polyether Glycols of 30 weight parts, 1 of 30 weight parts, hexamethylene-diisocyanate (HDI) joins thermometer is housed, in the there-necked flask of whipping appts and reflux condensing tube, under nitrogen protection, be heated to 90 ℃ of reaction 2h, then the dimethylol propionic acid DMPA reaction 1h that adds 3 weight parts, finally add 2 weight part chainextender N, N '-di-sec-butyl methylene dianiline (MDA), 60 ℃ of reaction 1h, be cooled to 30 ℃ of dischargings, triethylamine for performed polymer (TEA) is neutralized to pH=7, add again water-base epoxy Bao Zaiyin (Ag/EP-PEG) antiseptic-germicide 3 weight parts, deionized water 25 weight parts, emulsify at a high speed 30min obtains white emulsion.
The preparation of B component: add silicon powder 12 weight parts, titanium dioxide 8 weight parts, talcum powder 12 weight parts in Scattered Kettle, polyglycerol ether 25 weight parts, deionized water 30 weight parts, TriMethylolPropane(TMP) 2 weight parts, silicone antifoam agent 2 weight parts, polyether modified silicon oil flow agent 2 weight parts, poly carboxylic acid ammonium salt dispersion agent 2 weight parts, fire retardant hydrotalcite 5 weight parts, middling speed disperses, after 3h, then through sand mill, to be ground to granularity at 50um.In mixture, add mill base 5 weight parts again, high speed dispersion evenly obtains B component.
During use, B component is joined in component A by the weight ratio of 1:1, high-speed stirring 20min under normal temperature, with trowel or Cylinder coating brush in accomplishing fluently on the terrace of priming paint.
The auxiliary agents such as the defoamer using in the various embodiments described above, dispersion agent, flow agent are not limited to described several, and conventional auxiliary agent all can be used in the art.
Finally be necessary explanation: above embodiment is only for being described in further detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (7)
1. a high-efficiency antimicrobial aqueous polyurethane terrace paint, comprises A component and B component, it is characterized in that, described A component is comprised of the following raw material of counting by weight:
Described B component is comprised of the following raw material of counting by weight:
Wherein, the preparation method of described aqueous high molecular bag carrying nano silver antiseptic-germicide is: first by polyoxyethylene glycol, epoxy resin is carried out to modification, obtain water miscible modified epoxy, then described water miscible modified epoxy is not only as reductive agent but also as stablizer, water is reaction medium, and the method for reduction Silver Nitrate has obtained the water-base epoxy bag Ag-carried antibacterial agent emulsion of stably dispersing.
2. high-efficiency antimicrobial aqueous polyurethane terrace paint according to claim 1, it is characterized in that, described polyether glycol is selected from the polyether glycol that at least one or degree of unsaturation in the multipolymer of polyglycol ether, polypropylene glycol ether, polyglycerol ether, polypentaerythritol ether, PTMG, above-mentioned several polyether glycols are 1～4.
3. high-efficiency antimicrobial aqueous polyurethane terrace paint according to claim 1, is characterized in that: described color stuffing comprises at least one in silicon powder, titanium dioxide, talcum powder, wollastonite powder, calcium carbonate, barium sulfate, kaolin.
4. high-efficiency antimicrobial aqueous polyurethane terrace paint according to claim 1, is characterized in that: described chainextender comprises amine chain extender and alcohols chainextender.
5. high-efficiency antimicrobial aqueous polyurethane terrace paint according to claim 4, is characterized in that: described amine chain extender is selected from diethyl toluene diamine, diformazan sulfydryl tolylene diamine, N, at least one in N '-di-sec-butyl methylene dianiline (MDA); Described alcohols chainextender is selected from least one in BDO, 1,3 butylene glycol, TriMethylolPropane(TMP), glycerol, tetramethylolmethane.
6. high-efficiency antimicrobial aqueous polyurethane terrace paint according to claim 1, is characterized in that: described auxiliary agent is selected from least one in defoamer, thickening material, Ricinate, slip(ping)agent, flow agent.
7. a preparation method for high-efficiency antimicrobial aqueous polyurethane terrace paint as claimed in claim 1, is characterized in that,
The preparation method of described A component comprises the steps: under nitrogen protection, by 1, react hexamethylene-diisocyanate and polyether glycol mixing post-heating to 85～95 ℃, then adds dimethylol propionic acid reaction 1h, finally adds chainextender, 55～65 ℃ of reaction 4～6h, cooling rear discharging, obtains isocyanic ester performed polymer, by described isocyanic ester performed polymer with in triethylamine and after, add again water-based bag Ag-carried antibacterial agent emulsion, obtain A component product;
The preparation method of described B component comprises the steps: color stuffing, polyether glycol, chainextender, auxiliary agent, fire retardant to add in deionized water and mix, being ground to particle diameter is 30～50um, add again mill base, under 700～1500rpm rotating speed, stir and obtain B component, obtain B component product.
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| CN104559732A (en) * | 2015-01-09 | 2015-04-29 | 袁福德 | Method for preparing antibacterial and waterproof polyurethane coating and adhesive |
| CN104629606A (en) * | 2015-02-05 | 2015-05-20 | 金林墨 | Antibacterial waterproof polyurethane coating and preparation method thereof |
| CN104629607A (en) * | 2015-02-05 | 2015-05-20 | 林伊铭 | Environmental-friendly flame-retardant waterproof aqueous polyurethane coating and preparation method thereof |
| CN105384907A (en) * | 2015-11-09 | 2016-03-09 | 淄博德信联邦化学工业有限公司 | Low-odor and low-toxicity plastic floor elastic layer emulsion and preparation method thereof |
| CN106118434A (en) * | 2016-08-11 | 2016-11-16 | 王斐芬 | High ferro flame-proof antibiotic polyurethane water-proof paint |
| CN106147585A (en) * | 2016-08-11 | 2016-11-23 | 王斐芬 | High ferro Special high-strength water-repellent paint |
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| CN108530601A (en) * | 2018-03-30 | 2018-09-14 | 合肥科天水性科技有限责任公司 | A kind of nano silver aqueous polyurethane and preparation method thereof for from sterilization type thin-walled material |
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| CN111116859A (en) * | 2019-12-31 | 2020-05-08 | 杭州吉华高分子材料股份有限公司 | Preparation method of antibacterial modified waterborne polyurethane |
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| CN106147585B (en) * | 2016-08-11 | 2018-07-06 | 佛山市科妮迪新材料有限公司 | High ferro Special high-strength water-repellent paint |
| CN106118434A (en) * | 2016-08-11 | 2016-11-16 | 王斐芬 | High ferro flame-proof antibiotic polyurethane water-proof paint |
| CN106147585A (en) * | 2016-08-11 | 2016-11-23 | 王斐芬 | High ferro Special high-strength water-repellent paint |
| CN106280966A (en) * | 2016-08-11 | 2017-01-04 | 王斐芬 | High ferro flame-retardant waterproof coating |
| CN106280965A (en) * | 2016-08-11 | 2017-01-04 | 王斐芬 | Compound high iron waterproof material |
| CN106380919A (en) * | 2016-09-21 | 2017-02-08 | 苏州瑞斯格电子科技有限公司 | High-wear-resistant nanometer polyurethane floor paint |
| CN106947047A (en) * | 2017-03-31 | 2017-07-14 | 福建师范大学泉港石化研究院 | A kind of antibacterial aqueous polyurethane and its synthetic method |
| CN108219107A (en) * | 2018-01-11 | 2018-06-29 | 山东扬名新材料技术有限公司 | Anion aqueous polyurethane floor coatings resin |
| CN108530601A (en) * | 2018-03-30 | 2018-09-14 | 合肥科天水性科技有限责任公司 | A kind of nano silver aqueous polyurethane and preparation method thereof for from sterilization type thin-walled material |
| CN109439179A (en) * | 2018-12-17 | 2019-03-08 | 福州皇家地坪有限公司 | Aqueous polyurethane anti-corrosion floor material |
| CN110499060A (en) * | 2019-08-30 | 2019-11-26 | 深圳市威尔地坪材料有限公司 | A kind of elasticity antistatic polyurethane coating and its application |
| CN110862503A (en) * | 2019-11-29 | 2020-03-06 | 佛山市瑞福物联科技有限公司 | Preparation method of conductive polyurethane prepolymer and conductive adhesive thereof |
| CN110862503B (en) * | 2019-11-29 | 2022-02-11 | 佛山市瑞福物联科技有限公司 | Preparation method of conductive polyurethane prepolymer and conductive adhesive thereof |
| CN111116859A (en) * | 2019-12-31 | 2020-05-08 | 杭州吉华高分子材料股份有限公司 | Preparation method of antibacterial modified waterborne polyurethane |
| CN111116859B (en) * | 2019-12-31 | 2021-08-03 | 杭州吉华高分子材料股份有限公司 | Preparation method of antibacterial modified waterborne polyurethane |
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